3-(ethylamino)propane-1,2-diol synthesis
- Product Name:3-(ethylamino)propane-1,2-diol
- CAS Number:19737-19-0
- Molecular formula:C5H13NO2
- Molecular Weight:119.16
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Yield:-
Reaction Conditions:
in water;ethylamine;
Steps:
6 ?Example[6]
?Example[6] A 20-liter SUS316-made reaction vessel equipped with an agitator and a jacket was charged with 1600 g of monoethylamine aqueous solution having 70% by weight, followed by feeding 180 g of glycidol over 4 hours, and aging for 1 hour. Reaction temperature was controlled at 30° C. Concentration of monoethylamine and water in thus-obtained crude reaction liquid was 53.5% by weight and 26.0% by weight, respectively. The crude reaction liquid was fed into an apparatus (column size: 25 mm phi*900 mm H) equipped with a demister at an upper portion of a stainless-made falling-liquid film evaporator in feeding speed of 500 g/hour, and evaporation was carried out in column-top pressure of 760 Torr while heating at 102° C. Subsequently, a crude liquid discharged from the evaporator was introduced into the same distillation apparatus as in Example 1, followed by distilling at temperature of evaporating portion of 133° C. and in column-top pressure of 200 Torr to remove unreacted monoethylamine and water and to obtain a crude liquid. In the crude liquid, 1-monoethylamino-2,3-propanediol content was 80.4% by weight, water content was 1.0% by weight, and other ingredients content was 19.0% by weight. Subsequently, the crude liquid was fed into the same distillation apparatus as in Example 1 in feeding speed of 300 g/hour, and distillation was carried out at the temperature of 165° C. and pressure of 7.1 Torr at an evaporating portion, column-top pressure of 3.6 Torr and the temperature of 125° C. in the packed column top, and reflux ratio of 2. Vapor distilled out was introduced into a condenser to obtain a condensate at the temperature of 80° C. It is to be noted that steam pressure which is supplied into the jacket of the evaporating portion was controlled so that a yield of 1-monoethylamino-2,3-propanediol is adjusted to 95%. In the condensate obtained, color hue (APHA) was 10, water content was 0.07% by weight, and 1-monoethylamino-2,3-propanediol content was 99.6% by weight. Results are shown in Table 3.
References:
US5874624,1999,A
